HRID50200

反应详情

EQUATION

反应方程式

HRID 50200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.4 g (63 mmol) of 4-cyanophenoxyacetic acid were dissolved in 200 mL of absolute tetrahydrofuran and mixed at room temperature with 10.2 g (63 mmol) of N,N′-carbonyldiimidazole. After 15 minutes at 60° C., 5.70 g (41.5 mmol) of 2-amino-3-methylamino-6-methylpyridine were added. After 2 hours at 60° C., the solvent was distilled off and the crystalline residue was mixed with water, washed with water, and dried. After crystallization from ethanol, 9.95 g (91% of theory) were obtained in the form of white crystals. C16H14N4O (278.32). Mass spectrum: M+=278.

WORKUP

后处理

  1. waitAfter 2 hours at 60° C.
  2. distillationthe solvent was distilled off
  3. additionthe crystalline residue was mixed with water
  4. washwashed with water
  5. customdried
  6. customAfter crystallization from ethanol
  7. custom9.95 g (91% of theory) were obtained in the form of white crystals